EP3182147A1 - Readily accessible deep cooled nmr shim assembly - Google Patents

Abstract

A magnet assembly in an NMR apparatus comprising a superconducting magnet coil system (C) for producing a homogeneous He vessel (H1) with liquid helium and a He inner tube (H), the magnet coil system being mechanically rigidly connected to the He vessel wherein a radiation shield having a radiation shield inner tube (S) circumferentially surrounds the He container for reducing the rate of evaporation of the liquid helium, and wherein in the space between the He inner tube and the radiation shield inner tube, a field shaping device (P) of magnetic material for shining the homogeneous magnetic field is arranged, is characterized in that the field shaping device is fixed in the space between the He inner tube and the radiation shield inner tube so that it is in a rigid mechanical contact with the He container, without touching the radiation shield inner tube. The field shaping device may be installed in the cryostat such that it does not move relative to the superconducting coils. The He container need not be opened for work on the field forming device and disassembly of the cryostat is avoided.

Description

The invention relates to a magnet assembly in an NMR apparatus with a superconducting magnet coil system for generating a homogeneous magnetic field in the direction of a z-axis, wherein the magnet coil system in a He container with a He inner tube containing liquid helium during operation for cooling the coils is disposed and mechanically rigidly connected to the He container, wherein a radiation shield with a radiation shield inner tube surrounds the He container for reducing the evaporation rate of liquid helium at a distance, and wherein in the space between the He inner tube and the radiation shield inner tube, a field shaping device of soft magnetic Material for shimming the homogeneous magnetic field is arranged.

Such an arrangement is known from the JP 3737636 B2 ,

Background of the invention

The field of application of superconducting magnet systems comprises various fields of application, in particular magnetic resonance methods. In order to achieve a good resolution in such methods, the magnetic field in the sample volume must have a high degree of homogeneity. With the geometric arrangement of the field-generating magnetic coils, the basic homogeneity of the superconducting magnet can be optimized.

Frequently, in order to improve the magnetic field homogeneity, recesses are provided in the magnet coils (so-called notch structures) in which no wire is wound. However, valuable space for magnet windings is lost, making the magnet more expensive and increasing the stray field. In an arrangement according to US 6,617,853 B2 For example, a superconducting magnet for high resolution spectroscopy is made more compact by providing one or more soft magnetic rings which take on the role of certain notch structures in the magnetic coils.

wobei nach Design die Koeffizienten A_nm mit m≠0 und alle Koeffizienten B_nm verschwinden. Aufgrund von Fertigungstoleranzen in der Magnetanordnung weichen die Koeffizienten A_nm und B_nm vom berechneten Wert ab. Üblicherweise sind zur Korrektur dieser nicht verschwindenden Koeffizienten Shimspulen vorgesehen, die je mit einem eigenen Strom gespeist werden können. Bei großen Abweichungen der Koeffizienten von ihrem Sollwert kann es vorkommen, dass der in gewissen Shimspulen benötigte Strom zu hoch ist und das Magnetfeld der Magnetanordnung nicht wie gewünscht korrigiert werden kann. Alternativ dazu kann es vorkommen, dass der problematische Koeffizient in der Entwicklung des Magnetfelds nach Kugelfunktionen nicht korrigiert werden kann, weil gar keine Shimspule dafür vorgesehen ist. In einer solchen Situation ist eine teure Reparatur des Magnetsystems erforderlich, bei der ein Teil der Magnetanordnung ersetzt werden muss.The z-component of the magnetic field of an arrangement according to US 6,617,853 B2 can be developed in the sample volume according to spherical functions: $$B_z\left(r,z,\phi \right)={\displaystyle \underset{n=0}{\overset{\infty }{\Sigma }}}{\displaystyle \underset{m=0}{\overset{n}{\Sigma }}}{P}_n^m\left(\frac{z}{\sqrt{r^2+z^2}}\right){\left(r^2+z^2\right)}^{{}^n{/}_2}\left(A_{\mathit{nm}}\cos \left(\mathit{Mø}\right)+B_{\mathit{nm}}\sin \left(\mathit{Mø}\right)\right).$$

according to design, the coefficients A _nm with m ≠ 0 and all coefficients B _nm disappear. Due to manufacturing tolerances in the magnet arrangement, the coefficients A _nm and B _nm deviate from the calculated value. Usually Shimspulen are provided to correct these non-vanishing coefficients, which can each be fed with its own power. For large deviations of the coefficients from their nominal value, it may happen that the current required in certain shim coils is too high and the magnetic field of the magnet assembly can not be corrected as desired. Alternatively, it may happen that the problematic coefficient in the development of the magnetic field after spherical functions can not be corrected because no shim coil is provided for it. In such a situation, an expensive repair of the magnet system is required in which a part of the magnet assembly must be replaced.

In order to improve the magnetic field homogeneity without winding new magnetic coils, suitable soft magnetic field shaping devices may be provided.

In the DE 10 16 505 A1 various types of field forming devices made of sheet metal or foils are described. Special cases where the sheet or foils have cut out rectangular windows are described in US Pat JP 4384220 B2 listed. Not continuous holes in the sheet are also in the DE 10 2012 220 126 A1 disclosed.

Specially shaped field-forming devices may also have the purpose of eliminating the above-described notch structures in superconducting magnet coils to make the magnet more compact, such as in US Pat DE 10 104 054 C1 is explained.

In the cited above JP 3737636 B2 Another important aspect of field shaping devices is discussed: The saturation magnetization of the soft magnetic material is temperature dependent. This dependence is particularly pronounced at high temperatures, such as at room temperature. Small temperature fluctuations of the field shaping device then cause a field change in the working volume due to the variable saturation magnetization, which can affect the NMR measurement.

To counteract this, it is proposed that the field shaping device in He container to install. The low temperature of the field shaping device and its cooling by the liquid helium create ideal conditions for stable conditions. However, since the field shaping device can only be dimensioned after measuring the field in the working volume, the cryostat must be warmed up after a first magnetic test and completely disassembled before the field shaping device can be mounted in the He container. Such a step costs time and money.

Also the DE 10 2012 220 126 A1 As one possible solution, cooling of the field shaping device to the temperature of the liquid helium is suggested, thereby improving the magnetic properties of the field shaping device. As an alternative, in the DE 10 2012 220 126 A1 proposed an attachment of the field shaping device in an area located at room temperature of the magnet assembly so that the components of the field shaping device in the operating state from the outside are easily accessible and can be modified without warming the magnetic coil system.

As an alternative solution is in the cited above JP 3737636 B2 proposed to stick the field shaping device on the inner tube of the nitrogen container, which surrounds the He container. This inner tube has the task to keep the radiation of the room temperature inside tube from He container and is therefore also called radiation shield inner tube below. With a suitable construction of the cryostat then after a first magnetic test only a warm-up, but not a complete decomposition of the cryostat for attaching the field shaping device is required.

Unfortunately, this seemingly ideal solution has a big drawback, which the authors of the JP 3737636 B2 was overlooked: The nitrogen tank moves namely with changes in the nitrogen level and with him, of course, the inner tube with the mounted on Field forming device. However, this movement has now a very significant variation of the magnetic field homogeneity in the working volume result, which can not be accepted in many applications.

Object of the invention

The present invention is based on the object, in a superconducting magnet assembly with field shaping device of the type defined to increase the magnetic field homogeneity in the working volume with simple technical measures and without volume increase of the magnet assembly significantly, the field shaping device -something for retrofitting or Justierungzwecken- without a consuming disassembly of the cryostat, especially the He-container, or the magnet assembly should be easily accessible from the outside.

Brief description of the invention

This object is achieved in a surprisingly simple as well as effective manner by a magnet arrangement of the type mentioned, which is characterized in that the field shaping device is secured in the space between the He inner tube and the radiation shield inner tube so that they are in a rigid mechanical contact with the He container stands without touching the radiation shield inner tube. The present invention thus avoids the above-mentioned disadvantages of the prior art by mechanically decoupling the field shaping device from the nitrogen container but placing it outside the He container.

Further advantages over the prior art:

Since the superconducting magnet coil system is also rigidly connected to the He vessel, the relative movement of the field shaping device to the superconducting magnet coil system is inhibited, whereby the homogeneity in the working volume remains stable.

Good thermal contact of the field-shaping device with the He container is not absolutely necessary, since its temperature also sets without thermal contact with the He container due to the combined radiation of the He inner tube and the inner shield of the radiation shield. Both inner tubes are in the operating state at a very constant cryogenic temperature, which is why the temperature of the field shaping device also remains highly stable.

This allows a wealth of different mounting options of the field shaping device with the He container. The materials used in this case do not necessarily have a good thermal conductivity. Thermally poor contact surfaces are also permissible as long as the rigid mechanical connection with the He container is ensured.

Preferred embodiments and further developments of the invention

In most cryostats, the radiation shield inner tube is mechanically rigid and attached in thermal contact with a container of liquid nitrogen. The thermal contact gives the radiation shield inner tube its low temperature. This low temperature is critical for small radiation entries in the He vessel, minimizing He losses.

In other cryostats, the radiation shield inner tube is brought to its operating temperature by thermal contact with a cryocooler brought. This temperature can be even lower than that of the liquid nitrogen, which additionally reduces the He losses. Such cryostats also have the advantage of not requiring a volume of liquid nitrogen, allowing the design of more compact cryostats.

Also advantageous in a magnet arrangement according to the invention is a field shaping device which contains a cylindrical body of soft magnetic material. Such a body has the ideal shape to be positioned between the inner tube and the inner shield of the radiation shield. Also, the production of such a body is relatively simple.

Non-cylindrically symmetric recesses in the cylindrical body have the advantage of providing great flexibility for shimming the magnetic field in the working volume. These recesses may be continuous or not. Continuous recesses are easier to produce, but non-penetrating recesses give more scope for the design of the field shaping device.

• Eine Möglichkeit ist die Verwendung eines Stützrohrs, mittels dessen mindestens Teile der Feldformvorrichtung positioniert sind. In der Regel bestehen diese Teile aus einem oder mehreren Zylindern mit oder ohne Aussparungen. Vorzugsweise sind sie mit dem Stützrohr mechanisch gut verbunden. Bei Vertikalsystemen kann das Eigengewicht diese mechanische Verbindung sein. Bei Zylindern mit Aussparungen ist auch deren Orientierung wichtig. Eine formschlüssige Verbindung kann dafür eine Lösung sein.

The field-shaping device prescribed according to the invention must be arranged such that its position with respect to the superconducting magnet coil system always remains well-defined and remains constant over time in the operating state. For the realization of this condition there are several possibilities:

• One possibility is the use of a support tube, by means of which at least parts of the field shaping device are positioned. In general, these parts consist of one or more cylinders with or without recesses. Preferably, they are mechanically well connected to the support tube. For vertical systems, the dead weight can be this mechanical connection. For cylinders with recesses and their orientation is important. A positive connection can be a solution for this.

Alternatively, the support tube can also be soldered or glued to the cylinder (s). The support tube can for example be screwed to the bottom of the He container. Also solutions with a support tube on each side of the field shaping device are possible.

Another possibility is to connect at least parts of the field shaping device by means of a clamping mechanism with the He inner tube. In this solution can be dispensed with a support tube. With a suitable design, these parts of the field shaping device can be removed again if necessary.

In other embodiments of the invention, at least parts of the field shaping device may be glued to the outer surface of the He inner tube. This solution has the advantage that these parts of the field shaping device are mechanically stable with respect to the magnetic coil system. However, care must be taken that an adhesive is used which is suitable for low temperatures.

In further advantageous embodiments of the magnet arrangement according to the invention, the field shaping device contains at least one foil made of soft magnetic material which is arranged on a carrier tube. The support tube, like the support tube described above, is mechanically connected to the He container. Each foil of soft magnetic material can be customized, which gives more freedom in design than a solution with one or more cylinders.

The invention can be used particularly advantageously in a magnet coil system which contains at least one coil which is wound with high-temperature superconductor material. In the case of magnets with high-temperature superconductors, in particular strip conductors, poor homogeneity is a major problem. One reason is that the superconducting layer in these Conductors is typically several millimeters wide, so that the superconducting current can be distributed inhomogeneous. This results in greater field inhomogeneities in the working volume than in traditional low temperature superconductors in which the current-carrying filaments typically have a diameter of a few hundredths of a millimeter. In addition, the fact that the electric cryo-shims, which are used to improve the homogeneity, are located radially further from the magnetic axis than the high-temperature superconductor. When energized, a current is induced in the high-temperature superconductor that weakens the magnetic field of the shims in the working volume. Thus, the cryo-shims are often no longer able to compensate for the magnetic field inhomogeneity in the working volume and it must be sought for alternative solutions.

An embodiment in which the magnet coil system has an active shield is also preferred. This active shield reduces the stray field of the magnet assembly, leaving more room in the lab for other applications.

Also advantageous is an embodiment of the magnet arrangement according to the invention, in which the field shaping device is magnetically completely saturated and magnetized purely axially (in one direction along the z-axis). In this situation, the calculation of the field produced by the field shaping device is particularly simple and accurate.

Also advantageous is an embodiment of the magnet arrangement according to the invention, in which parts of the field shaping device have been subjected to a surface treatment, in particular that they have been galvanized. This surface treatment offers optimum protection against corrosion, which is essential in particular for parts made of soft iron.

A particularly preferred embodiment of the magnet arrangement according to the invention is characterized in that the field shaping device comprises a plurality of magnetic material elements. This offers more degrees of freedom for optimizing the field shaping device.

The scope of the present invention also includes a method for producing a magnet arrangement of the type according to the invention described above, which is characterized in that at least a part of the non-cylindrically symmetrical recesses is removed by spark erosion. With spark erosion high mechanical accuracy can be achieved.

Alternatively, it can be provided in another variant of the method that at least a portion of the non-cylindrically symmetrical recesses is removed by a corrosive substance. By suitably covering areas of the field shaping device that do not need to be reworked, material can be easily removed by an etching process in an acid bath. The etching time must be adjusted so that the correct thickness of material is removed.

Another alternative is a variant of the method in which at least a portion of the non-cylindrically symmetrical recesses is removed by electrolysis. Instead of an acid bath as in the above process variant, an electrolyte bath is used here.

Finally, in a further variant of the method at least a portion of the non-cylindrically symmetrical recesses can also be removed by means of grinding or milling. Grinding and milling are ancient procedures that are mastered by every precision mechanic. There is also no need for any special equipment for carrying out these processes.

In embodiments of the magnet arrangement according to the invention, which have non-cylindrically symmetrical recesses in the form of through holes through the field shaping device, the holes can also be cut out with a laser beam. A major advantage of the laser method is the very high mechanical precision, so that even complicated predetermined shapes can be produced extremely accurately.

Further advantages of the invention will become apparent from the description and the drawings. Likewise, according to the invention, the above-mentioned features and those which are still further developed can each be used individually for themselves or for a plurality of combinations of any kind. The embodiments shown and described are not to be understood as exhaustive enumeration, but rather have exemplary character for the description of the invention.

Detailed description of the invention and drawing

Fig. 1

einen schematischen Vertikalschnitt durch eine radiale Hälfte der erfindungsgemäßen Magnetanordnung, bei der die Feldformvorrichtung mittels eines Stützrohrs mit dem Boden des Heliumbehälters fixiert ist

Fig. 2

ein Stützrohr mit einer Feldformvorrichtung ;

Fig. 3

einen schematischen Vertikalschnitt durch eine radiale Hälfte der erfindungsgemäßen Magnetanordnung, bei der die Feldformvorrichtung mittels eines Klemmmechanismus mit dem He-Innenrohr fixiert ist;

Fig. 4

einen schematischen Vertikalschnitt durch eine radiale Hälfte der erfindungsgemäßen Magnetanordnung, bei der die Feldformvorrichtung Folien enthält, die auf einem Trägerrohr liegen, welcher mit dem Boden des Heliumbehälters fixiert ist;

Fig. 5

einen schematischen Vertikalschnitt durch eine radiale Hälfte der erfindungsgemäßen Magnetanordnung mit einem He-Behälter, einem Strahlungsschildbehälter und einem Behälter mit flüssigem Stickstoff;

Fig. 6

einen schematischen Vertikalschnitt durch eine radiale Hälfte der erfindungsgemäßen Magnetanordnung mit einem He-Behälter und einem Strahlungsschildbehälter, welcher mit einem Kryokühler auf seine Betriebstemperatur gebracht wird;

Fig. 7

eine Feldformvorrichtung mit durchgängigen Aussparungen; und

Fig. 8

eine Feldformvorrichtung mit nicht-durchgängigen Aussparungen.

The invention is illustrated in the drawing and will be explained in more detail with reference to embodiments. Show it:

Fig. 1

a schematic vertical section through a radial half of the magnet arrangement according to the invention, in which the field-shaping device is fixed by means of a support tube to the bottom of the helium container

Fig. 2

a support tube with a field forming device;

Fig. 3

a schematic vertical section through a radial half of the magnet arrangement according to the invention, in which the field shaping device by means of a clamping mechanism with the He inner tube is fixed;

Fig. 4

a schematic vertical section through a radial half of the magnet arrangement according to the invention, in which the field shaping device contains films which lie on a support tube which is fixed to the bottom of the helium container;

Fig. 5

a schematic vertical section through a radial half of the magnet assembly according to the invention with a He container, a radiation shield container and a container with liquid nitrogen;

Fig. 6

a schematic vertical section through a radial half of the magnet assembly according to the invention with a He container and a radiation shield container, which is brought with a cryocooler to its operating temperature;

Fig. 7

a field forming device with continuous recesses; and

Fig. 8

a field forming device with non-continuous recesses.

The FIG. 1 shows a schematic vertical section through a radial half of the magnet arrangement according to the invention, in which the field shaping device P is fixed by means of a support tube P0 to the bottom of the helium container. The superconducting magnet coil system C is mechanically rigidly connected to the bottom of the He vessel H1. The support tube P0 can for example be screwed or glued to the bottom of the He container. The screw connection is, however, more advantageous because it can be released again. The field shaping device P can be soldered to the support tube P0 or to be glued. Also a bayonet lock is conceivable. Alternatively, the field shaping device P can be clamped between two support tubes.

In the FIG. 2 For example, a support tube P0 and a field forming device P are shown prior to installation. The field shaping device P is in this example a cylinder with recesses A.

The FIG. 3 shows a schematic vertical section through a radial half of the magnet arrangement according to the invention, in which the field shaping device P is fixed by means of a clamping mechanism P1 with the He inner tube H. In this arrangement, no support tube is required. The clamping mechanism P1 may be made of either the same or a different material than the field shaping device P. If the same material is selected, the field forming device P and the clamping mechanism P1 can be made of a single workpiece. However, the influence of the clamping mechanism P1 on the magnetic field homogeneity in the working volume must be taken into account in the design of the field shaping device P.

The FIG. 4 shows a schematic vertical section through a radial half of the magnet arrangement according to the invention, in which the field shaping device P contains films which lie on a support tube P0, which is fixed to the bottom of the helium container. It is also possible to arrange a plurality of films one above the other on the support tube, preferably with a low-temperature adhesive tape. The slides can take on different shapes. For example, you can have holes with different patterns. You can cover the entire circumference of the support tube or only part of it. The carrier tube preferably includes a recess for the attachment of soft magnetic film. This ensures that the soft magnetic film remains intact during insertion of the support tube. The FIG. 5 shows a schematic vertical section through a radial half of the magnet arrangement according to the invention with a superconducting magnet coil system C, a He container H1, a radiation shield container S2 and a container S1 with liquid nitrogen. The radiation shield inner tube S in this case does not belong to the radiation shield container S2, but is connected in a heat-conducting manner to the nitrogen container S1. A room temperature container R1 with inner tube R surrounds the nitrogen tank S1. During operation, there is a vacuum in the spaces between the containers. The axis of symmetry z of the superconducting magnet coil system C and the working volume AV about the plane z = 0 are also shown.

The FIG. 6 shows a schematic vertical section through a radial half of the magnet arrangement according to the invention with a superconducting magnet coil system C, a He container H1 and a radiation shield container S2, which is brought to its operating temperature with a cryocooler CC. The radiation shield container S2 is thermally connected to a radiation shield inner tube S. As in the previous figure, the room temperature container R1 with inner tube R, the axis of symmetry z and the working volume AV around the plane z = 0 are also shown.

In the FIG. 7 is a field shaping device P with continuous recesses A shown. The recesses A are determined in shape and size so that the magnetic field in the working volume is as homogeneous as possible.

Finally, the shows FIG. 8 a field shaping device P with non-continuous recesses A. These can be produced for example by an etching process or by spark erosion.

LIST OF REFERENCE NUMBERS

C

Magnet coil system

H

He-inner tube

H1

He-container

S

Radiation shield inner tube

S1

Container with liquid nitrogen

S2

Radiation shield container

P

Field shaping device

P0

Support tube, support tube

P1

clamping mechanism

A

recess

AV

workload

R

Room temperature inner pipe

R1

Room temperature Bottles

CC

cryocooler

Claims (10)

Magnet arrangement in an NMR apparatus with a superconducting magnet coil system (C) for generating a homogeneous magnetic field in the direction of a z-axis, wherein the magnet coil system (C) in a He container (H1) with a He inner tube (H) in the Operation liquid helium for cooling the coils contains, arranged and mechanically rigidly connected to the He container (H1), wherein a radiation shield with a radiation shield inner tube (S) surrounds the He container (H1) with distance to reduce the evaporation rate of the liquid helium and wherein in the space between the He inner tube (H) and the radiation shield inner tube (S) is arranged a field shaping device (P) of magnetic material for shining the homogeneous magnetic field,
characterized,
that the field shaping device (P) is fixed in such a manner in the space between the He inner tube (H) and the radiation shield inner tube (S), that it is in a rigid mechanical contact with the He-container (H1) without the radiation shield inner tube (S) to touch. Magnet arrangement according to claim 1, characterized in that the radiation shield inner tube (S) is fixed mechanically rigidly on and in thermal contact with a container (S1) with liquid nitrogen. Magnet arrangement according to claim 1, characterized in that a cryocooler (CC) is present, by means of which the radiation shield inner tube (S) can be brought to its operating temperature by thermal contact. Magnet arrangement according to one of the preceding claims, characterized in that the field shaping device (P) has a cylindrical Contains body of soft magnetic material. Magnet arrangement according to Claim 4, characterized in that the cylindrical body of the field-shaping device (P) has non-cylindrically symmetrical recesses (A). Magnet arrangement according to one of the preceding claims, characterized in that at least parts of the field shaping device (P) by means of a support tube (P0) are positioned. Magnet arrangement according to one of the preceding claims, characterized in that at least parts of the field shaping device (P) by means of a clamping mechanism (P1) with the He inner tube (H) are connected. Magnet arrangement according to one of the preceding claims, characterized in that at least parts of the field shaping device (P) with the outer surface of the He inner tube (H) are bonded. Magnet arrangement according to one of the preceding claims, characterized in that the field shaping device (P) comprises at least one foil of soft magnetic material, which is arranged on a support tube (P0). Magnet arrangement according to one of the preceding claims, characterized in that the superconducting magnet coil system (C) comprises at least one coil which is wound with high-temperature superconductor material.

Images